#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:37:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179386 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/83/4328382.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4328382
loop_
_publ_author_name
'Qing-Yan Liu'
'Wu-Fang Wang'
'Yu-Ling Wang'
'Zeng-Mei Shan'
'Ming-Sheng Wang'
'Jinkui Tang'
_publ_contact_author_address
;
College of Chemistry and Chemical Engineering,
Jiangxi Normal University,
Nanchang, Jiangxi 330022,
P. R. China
;
_publ_contact_author_email       qyliuchem@hotmail.com
_publ_contact_author_fax         +86-791-88120387
_publ_contact_author_name        'Qing-Yan Liu'
_publ_contact_author_phone       +86-791-88120387
_publ_section_title
;
 Diversity of Lanthanide(III)-Organic Extended Frameworks with a
 4,8-Disulfonyl-2,6-naphthalenedicarboxylic Acid Ligand: Syntheses,
 Structures, and Magnetic and Luminescent Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2381
_journal_page_last               2392
_journal_paper_doi               10.1021/ic2023727
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C12 H28 O23 Pr2 S2'
_chemical_formula_weight         886.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.859(4)
_cell_length_b                   11.5288(18)
_cell_length_c                   21.861(3)
_cell_measurement_reflns_used    1449
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.64
_cell_volume                     5509.1(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0839
_diffrn_reflns_av_sigmaI/netI    0.0931
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11187
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    3.742
_exptl_absorpt_correction_T_max  0.6037
_exptl_absorpt_correction_T_min  0.5071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.137
_exptl_crystal_description       block
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.221
_refine_diff_density_min         -1.465
_refine_diff_density_rms         0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0619P)²+72.5748P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1389
_reflns_number_gt                2437
_reflns_number_total             3540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2023727_si_001_1.cif
_cod_data_source_block           Pr
_cod_original_cell_volume        5509.1(16)
_cod_database_code               4328382
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pr1 Pr 0.0000 0.04248(5) 0.65343(3) 0.01340(17) Uani 1 2 d S
Pr2 Pr -0.09344(3) -0.18290(5) 0.7500 0.01702(18) Uani 1 2 d S
S1 S -0.32982(12) -0.30994(19) 0.63205(10) 0.0235(5) Uani 1 1 d .
O1 O -0.1256(3) -0.1253(6) 0.6515(3) 0.0341(17) Uani 1 1 d .
O1W O -0.3299(5) 0.0271(8) 0.6102(5) 0.078(3) Uani 1 1 d .
O2 O -0.0634(3) -0.0698(5) 0.5765(3) 0.0235(14) Uani 1 1 d .
O2W O -0.4043(7) -0.1112(11) 0.7500 0.075(4) Uani 1 2 d S
O3 O -0.3904(3) -0.3585(6) 0.6370(3) 0.0310(16) Uani 1 1 d .
O3W O -0.3942(9) 0.0000 0.5000 0.113(7) Uani 1 2 d S
O4 O -0.3255(4) -0.1936(6) 0.6562(3) 0.048(2) Uani 1 1 d .
O4W O 0.0000 0.3792(13) 0.5486(11) 0.141(8) Uani 1 2 d S
O5 O -0.2829(4) -0.3854(7) 0.6577(3) 0.0433(19) Uani 1 1 d .
O6 O 0.0000 -0.1597(6) 0.6889(3) 0.0169(18) Uani 1 2 d S
H6 H 0.0000 -0.1933 0.6543 0.025 Uiso 1 2 d SR
O7 O -0.0601(4) 0.0236(6) 0.7500 0.0160(17) Uani 1 2 d S
H7 H -0.0942 0.0589 0.7500 0.024 Uiso 1 2 d SR
O8 O 0.0000 0.1439(7) 0.5490(4) 0.025(2) Uani 1 2 d S
O9 O 0.0000 0.2603(8) 0.6778(6) 0.047(3) Uani 1 2 d S
O10 O -0.1912(5) -0.0524(8) 0.7500 0.033(2) Uani 1 2 d S
O11 O -0.1940(5) -0.3037(10) 0.7500 0.055(3) Uani 1 2 d S
O12 O -0.0769(5) -0.3717(7) 0.6836(6) 0.092(4) Uani 1 1 d .
C1 C -0.1122(4) -0.1142(7) 0.5952(4) 0.0213(19) Uani 1 1 d .
C2 C -0.1583(4) -0.1587(7) 0.5510(4) 0.0206(19) Uani 1 1 d .
C3 C -0.2120(4) -0.2045(7) 0.5718(4) 0.0196(19) Uani 1 1 d .
H3A H -0.2194 -0.2051 0.6137 0.024 Uiso 1 1 calc R
C4 C -0.2563(4) -0.2505(7) 0.5325(4) 0.0185(18) Uani 1 1 d .
C5 C -0.3123(4) -0.3012(7) 0.5524(4) 0.0195(19) Uani 1 1 d .
C6 C -0.3532(4) -0.3448(7) 0.5123(4) 0.0200(19) Uani 1 1 d .
H6A H -0.3894 -0.3775 0.5267 0.024 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O6 Pr1 O7 69.5(2) . 3_556
O6 Pr1 O7 69.5(2) . .
O7 Pr1 O7 63.5(3) 3_556 .
O6 Pr1 O2 74.0(2) . .
O7 Pr1 O2 143.5(2) 3_556 .
O7 Pr1 O2 103.2(2) . .
O6 Pr1 O2 74.0(2) . 12
O7 Pr1 O2 103.2(2) 3_556 12
O7 Pr1 O2 143.5(2) . 12
O2 Pr1 O2 66.3(3) . 12
O6 Pr1 O8 135.5(3) . .
O7 Pr1 O8 142.45(19) 3_556 .
O7 Pr1 O8 142.45(19) . .
O2 Pr1 O8 69.0(2) . .
O2 Pr1 O8 69.0(2) 12 .
O6 Pr1 O9 149.6(3) . .
O7 Pr1 O9 84.8(3) 3_556 .
O7 Pr1 O9 84.8(3) . .
O2 Pr1 O9 129.6(2) . .
O2 Pr1 O9 129.6(2) 12 .
O8 Pr1 O9 74.9(3) . .
O6 Pr1 O3 116.54(15) . 16_455
O7 Pr1 O3 128.4(2) 3_556 16_455
O7 Pr1 O3 71.4(2) . 16_455
O2 Pr1 O3 68.9(2) . 16_455
O2 Pr1 O3 128.1(2) 12 16_455
O8 Pr1 O3 71.71(16) . 16_455
O9 Pr1 O3 67.10(16) . 16_455
O6 Pr1 O3 116.54(15) . 5
O7 Pr1 O3 71.4(2) 3_556 5
O7 Pr1 O3 128.4(2) . 5
O2 Pr1 O3 128.1(2) . 5
O2 Pr1 O3 68.9(2) 12 5
O8 Pr1 O3 71.71(16) . 5
O9 Pr1 O3 67.10(16) . 5
O3 Pr1 O3 126.9(3) 16_455 5
O6 Pr1 Pr2 36.99(9) . .
O7 Pr1 Pr2 76.16(16) 3_556 .
O7 Pr1 Pr2 38.08(16) . .
O2 Pr1 Pr2 74.57(14) . .
O2 Pr1 Pr2 107.66(13) 12 .
O8 Pr1 Pr2 141.36(11) . .
O9 Pr1 Pr2 122.4(2) . .
O3 Pr1 Pr2 83.62(15) 16_455 .
O3 Pr1 Pr2 145.15(15) 5 .
O6 Pr1 Pr2 36.99(9) . 3_556
O7 Pr1 Pr2 38.08(16) 3_556 3_556
O7 Pr1 Pr2 76.16(16) . 3_556
O2 Pr1 Pr2 107.66(13) . 3_556
O2 Pr1 Pr2 74.57(14) 12 3_556
O8 Pr1 Pr2 141.36(11) . 3_556
O9 Pr1 Pr2 122.4(2) . 3_556
O3 Pr1 Pr2 145.15(15) 16_455 3_556
O3 Pr1 Pr2 83.62(15) 5 3_556
Pr2 Pr1 Pr2 62.77(2) . 3_556
O1 Pr2 O1 131.6(3) 10_557 .
O1 Pr2 O6 73.8(2) 10_557 10_557
O1 Pr2 O6 135.5(2) . 10_557
O1 Pr2 O6 135.5(2) 10_557 .
O1 Pr2 O6 73.8(2) . .
O6 Pr2 O6 65.9(3) 10_557 .
O1 Pr2 O7 79.53(19) 10_557 .
O1 Pr2 O7 79.53(19) . .
O6 Pr2 O7 69.6(2) 10_557 .
O6 Pr2 O7 69.6(2) . .
O1 Pr2 O11 84.2(2) 10_557 .
O1 Pr2 O11 84.2(2) . .
O6 Pr2 O11 139.6(2) 10_557 .
O6 Pr2 O11 139.6(2) . .
O7 Pr2 O11 139.4(4) . .
O1 Pr2 O10 66.07(17) 10_557 .
O1 Pr2 O10 66.07(17) . .
O6 Pr2 O10 128.1(2) 10_557 .
O6 Pr2 O10 128.1(2) . .
O7 Pr2 O10 71.9(3) . .
O11 Pr2 O10 67.5(4) . .
O1 Pr2 O12 140.7(3) 10_557 .
O1 Pr2 O12 76.8(3) . .
O6 Pr2 O12 106.0(3) 10_557 .
O6 Pr2 O12 71.2(3) . .
O7 Pr2 O12 138.4(3) . .
O11 Pr2 O12 71.0(3) . .
O10 Pr2 O12 125.9(3) . .
O1 Pr2 O12 76.8(3) 10_557 10_557
O1 Pr2 O12 140.7(3) . 10_557
O6 Pr2 O12 71.2(3) 10_557 10_557
O6 Pr2 O12 106.0(3) . 10_557
O7 Pr2 O12 138.4(3) . 10_557
O11 Pr2 O12 71.0(3) . 10_557
O10 Pr2 O12 125.9(3) . 10_557
O12 Pr2 O12 66.7(6) . 10_557
O1 Pr2 Pr1 58.52(17) 10_557 10_557
O1 Pr2 Pr1 117.38(18) . 10_557
O6 Pr2 Pr1 37.03(16) 10_557 10_557
O6 Pr2 Pr1 77.71(16) . 10_557
O7 Pr2 Pr1 38.18(9) . 10_557
O11 Pr2 Pr1 142.61(14) . 10_557
O10 Pr2 Pr1 92.55(19) . 10_557
O12 Pr2 Pr1 140.4(3) . 10_557
O12 Pr2 Pr1 100.3(2) 10_557 10_557
O1 Pr2 Pr1 117.38(18) 10_557 .
O1 Pr2 Pr1 58.52(17) . .
O6 Pr2 Pr1 77.71(16) 10_557 .
O6 Pr2 Pr1 37.03(16) . .
O7 Pr2 Pr1 38.18(9) . .
O11 Pr2 Pr1 142.61(14) . .
O10 Pr2 Pr1 92.55(19) . .
O12 Pr2 Pr1 100.3(2) . .
O12 Pr2 Pr1 140.4(3) 10_557 .
Pr1 Pr2 Pr1 65.14(2) 10_557 .
O1 Pr2 Pr2 107.34(17) 10_557 3_556
O1 Pr2 Pr2 107.34(17) . 3_556
O6 Pr2 Pr2 33.69(15) 10_557 3_556
O6 Pr2 Pr2 33.69(15) . 3_556
O7 Pr2 Pr2 72.96(18) . 3_556
O11 Pr2 Pr2 147.6(3) . 3_556
O10 Pr2 Pr2 144.9(2) . 3_556
O12 Pr2 Pr2 82.1(3) . 3_556
O12 Pr2 Pr2 82.1(3) 10_557 3_556
Pr1 Pr2 Pr2 58.614(12) 10_557 3_556
Pr1 Pr2 Pr2 58.614(12) . 3_556
O3 S1 O4 113.2(5) . .
O3 S1 O5 112.7(4) . .
O4 S1 O5 111.6(5) . .
O3 S1 C5 107.0(4) . .
O4 S1 C5 106.8(4) . .
O5 S1 C5 104.9(4) . .
C1 O1 Pr2 147.3(7) . .
C1 O2 Pr1 117.3(5) . .
S1 O3 Pr1 175.7(4) . 5_445
Pr2 O6 Pr2 112.6(3) 3_556 .
Pr2 O6 Pr1 105.98(19) 3_556 .
Pr2 O6 Pr1 105.98(19) . .
Pr2 O6 H6 115.7 3_556 .
Pr2 O6 H6 115.7 . .
Pr1 O6 H6 98.7 . .
Pr2 O7 Pr1 103.74(19) . 10_557
Pr2 O7 Pr1 103.74(19) . .
Pr1 O7 Pr1 115.5(3) 10_557 .
Pr2 O7 H7 101.5 . .
Pr1 O7 H7 114.8 10_557 .
Pr1 O7 H7 114.8 . .
O2 C1 O1 123.6(8) . .
O2 C1 C2 120.4(8) . .
O1 C1 C2 116.0(8) . .
C3 C2 C6 119.6(8) . 13_446
C3 C2 C1 119.9(8) . .
C6 C2 C1 120.6(8) 13_446 .
C2 C3 C4 122.5(8) . .
C2 C3 H3A 118.8 . .
C4 C3 H3A 118.8 . .
C3 C4 C5 124.3(8) . .
C3 C4 C4 117.8(10) . 13_446
C5 C4 C4 117.9(9) . 13_446
C6 C5 C4 121.6(8) . .
C6 C5 S1 118.0(7) . .
C4 C5 S1 120.4(6) . .
C5 C6 C2 120.6(8) . 13_446
C5 C6 H6A 119.7 . .
C2 C6 H6A 119.7 13_446 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pr1 O6 2.457(7) .
Pr1 O7 2.495(4) 3_556
Pr1 O7 2.495(4) .
Pr1 O2 2.534(6) .
Pr1 O2 2.534(6) 12
Pr1 O8 2.565(9) .
Pr1 O9 2.567(9) .
Pr1 O3 2.679(7) 16_455
Pr1 O3 2.679(7) 5
Pr1 Pr2 3.9216(8) .
Pr1 Pr2 3.9216(8) 3_556
Pr2 O1 2.361(6) 10_557
Pr2 O1 2.361(6) .
Pr2 O6 2.455(4) 10_557
Pr2 O6 2.455(4) .
Pr2 O7 2.490(7) .
Pr2 O11 2.602(10) .
Pr2 O10 2.613(10) .
Pr2 O12 2.641(8) .
Pr2 O12 2.641(8) 10_557
Pr2 Pr1 3.9216(8) 10_557
Pr2 Pr2 4.0848(16) 3_556
S1 O3 1.441(7) .
S1 O4 1.444(7) .
S1 O5 1.458(8) .
S1 C5 1.785(8) .
O1 C1 1.271(11) .
O2 C1 1.252(11) .
O3 Pr1 2.679(7) 5_445
O6 Pr2 2.455(4) 3_556
O6 H6 0.8500 .
O7 Pr1 2.495(4) 10_557
O7 H7 0.8498 .
C1 C2 1.488(12) .
C2 C3 1.366(12) .
C2 C6 1.406(12) 13_446
C3 C4 1.400(11) .
C3 H3A 0.9300 .
C4 C5 1.424(12) .
C4 C4 1.449(16) 13_446
C5 C6 1.350(12) .
C6 C2 1.406(12) 13_446
C6 H6A 0.9300 .
